Hydrochloric Acid → HCID 67367219, compound

Temperature

25 °C

1-[6-(Azetidin-1-yl-methyl)-1,2,3,4-tetrahydro-isoquinolin-2-yl]-2,2,2-trifluoro-ethanone (5.162 mmol, 1 equiv.) was dissolved in methanol (20 ml); K2CO3 (10.32 mmol, 2 equiv.) was added, and the mixture was stirred for 1 hour at 25° C. Methanol was concentrated in vacuo, and the residue was taken up in dichloromethane (30 ml) and washed with distilled water (5 ml). The aqueous phase was extracted with DCM (20 ml), and the combined organic phases were dried over sodium sulfate and concentrated in vacuo. For purification, the crude product was dissolved in diethyl ether (50 ml), and a hydrochloride was precipitated with 2 M HCl in diethyl ether solution (3 equiv.). The hydrochloride was filtered off, washed with diethyl ether and dried in vacuo to yield the desired product. Yield: 1.03 g (73%)

1. concentrationMethanol was concentrated in vacuo
2. washwashed with distilled water (5 ml)
3. extractionThe aqueous phase was extracted with DCM (20 ml)
4. dry with materialthe combined organic phases were dried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customFor purification
7. dissolutionthe crude product was dissolved in diethyl ether (50 ml)
8. filtrationThe hydrochloride was filtered off
9. washwashed with diethyl ether
10. customdried in vacuo

ORD record

ord-29444be8927343398dcb76f998c7e3da

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08269000B2